CN101323457B - Method for preparing potassium muriate by using sea water - Google Patents
Method for preparing potassium muriate by using sea water Download PDFInfo
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- CN101323457B CN101323457B CN 200810053957 CN200810053957A CN101323457B CN 101323457 B CN101323457 B CN 101323457B CN 200810053957 CN200810053957 CN 200810053957 CN 200810053957 A CN200810053957 A CN 200810053957A CN 101323457 B CN101323457 B CN 101323457B
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Abstract
The invention relates to a new method for using seawater and the brine of the seawater as raw material to produce potassium chloride; concentration techniques of normal-temperature adsorption, elutionand regeneration are adopted, decomposition liquid and washing liquid are recycled to realize producing the potassium chloride by utilizing the seawater, with low energy consumption and low cost. Natural zeolite is used for adsorbing potassium in the seawater; a magnesium chloride solution containing ammonium chloride is used as an eluent and elution is carried out to prepare mother liquid rich inpotassium which contains the potassium, ammonium and magnesium; the mother liquid rich in potassium is evaporated and cooled to prepare a carnallite containing the ammonium and the magnesium chloride solution; water is added into the carnallite containing the ammonium to prepare the potassium chloride product and the magnesium chloride solution is added with the ammonium chloride to be used as th e eluent to return a elution system. The recovery rate of K<+> from self-evaporation and concentration to decomposition and washing processes in the technique recycling test is up to 85 percent and the product quality of the potassium chloride reaches first-class standard in III-class of GB6549-1996 potassium chloride.
Description
Technical field
The present invention relates to the preparation technique of Repone K in the field of inorganic chemical engineering, particularly utilize seawater to produce the method for Repone K for raw material.
Background technology
Repone K is the main kind of potash fertilizer, is in great demand.China's potassium resource scarcity, the potash fertilizer demand gap is bigger, and the annual import potash fertilizer that needs accounts for 70% of domestic apparent consumption more than 7,000,000 tons.Contain abundant potassium in the seawater, utilize seawater to extract potash fertilizer, be considered to alleviate the important channel that China's potassium resource lacks.
The potassium from sea water technology obtains paying attention in the marine chemical industry industry all the time, has carried out many-sided research and exploration.The processing method of the potassium from sea water of now having studied and having tested has: chemical precipitation method, organic solvent method, membrane separation process and inorganic ion exchanger method etc.
Chemical precipitation method is utilized the potassium ion combination in precipitation agent and the seawater, generates the extremely low sylvite precipitation of solubleness.Precipitation agent can pollute seawater, and extraction cost is also high proposing the loss of potassium process, and therefore, chemical precipitation method is under test substantially, fails to realize industrial production.
Organic solvent method comprises solvent extration, solvent precipitation, and employed organic solvent also with the seawater discharging, can pollute ocean environment, and the loss of solvent makes the production cost of potassium from sea water improve again.
Membrane separation process utilizes the difference in functionality and the characteristic of film, reaches the separation of different substances and the purpose of enrichment, and still, separation potassium effect is still undesirable, is in the exploratory stage.
The inorganic ion exchanger method is utilized the potassium ion in the mineral ion adsorbents adsorb seawater, will become Repone K under the potassium ion wash-out with chlorate again.The mineral ion sorbent material that is adopted mainly comprises phosphoric acid salt, silico-aluminate and the natural zeolite of synthetic.Because the inorganic ion exchanger low price has the selection exchangeability to potassium, is considered to the most promising potassium from sea water method.Particularly natural zeolite is not only cheap, and higher selectivity and exchange capacity are arranged, and can use repeatedly, in the use ocean environment and the eubiosis is had no adverse effects, and has therefore represented the good prospect of utilizing.
Natural zeolite method potassium from sea water adopts using natural clinoptilolite as the mineral ion sorbent material, direct k adsorption ion from seawater, be that 85～100 ℃ hot saturated brine is an eluent with being heated to temperature again, the rich potassium liquid behind the wash-out separates through evaporation and makes Repone K and two kinds of products of purified salt.But above-mentioned used eluent is to be heated to 85～100 ℃ saturated brine, and evaporates the evaporation of separation need than juicy, and therefore, the energy consumption of producing Repone K is higher, and the production cost of Repone K is higher than sale price on the market, is difficult to industrialization.
For above-mentioned natural zeolite method potassium from sea water, in order to reduce the cost that extracts Repone K, the mixture that adopts ammonium chloride and sodium-chlor is as eluent, at normal temperatures wash-out.But, the normal temperature wash-out of employing ammonium chloride and sodium chloride mixture, evaporation separates the nitrogen potassium that can only make KCE content about about 5% and mixes fertilizer, can't produce the Repone K that is up to state standards.
Summary of the invention
Utilize seawater to extract potash fertilizer at prior art and have energy consumption and the high problem of cost, the present invention is on the basis of natural zeolite method potassium from sea water, mixing solutions with magnesium chloride and ammonium chloride is made eluent, with the saturated brine is regenerator, adopt normal temperature absorption, wash-out and regenerated process of enriching, realize utilizing seawater less energy-consumption and low cost to produce Repone K.
The method of utilizing seawater to produce Repone K involved in the present invention comprises: with the potassium in the natural zeolite adsorbing seawater; To contain magnesium chloride and ammonium chloride mixing solutions is eluent, and the normal temperature wash-out is inhaled saspachite, makes the rich potassium mother liquor that contains potassium, magnesium, ammonium, chlorion; Rich potassium mother liquid evaporation concentrates, and complete evaporation of liquid cooling, centrifugation get carnallitite and magnesium chloride solution; Carnallitite adds water decomposition and gets Repone K and decomposed solution, and decomposed solution is evaporated again to reclaim the Repone K in the decomposed solution again.
Technical process of the present invention and processing parameter are as follows:
It is raw material that the present invention adopts seawater, is inorganic ion exchanger with the using natural clinoptilolite.For convenience of explanation, represent the solid skeletal of natural zeolite with Z, then NaZ represents na-pretreated zeolite, and KZ represents potassium type zeolite, NH
4Z represents ammonium type zeolite.
(1) absorption
Seawater is fed the using natural clinoptilolite of sodium type, then potassium ion K in the seawater
+Be adsorbed on the zeolite K
+With other ion initial gross separation, na-pretreated zeolite becomes potassium type zeolite.
Seawater+NaZ → suction back seawater+KZ
Seawater is the clarifying natural sea-water of precipitation, and adsorption temp is an outside temperature, and its temperature range is between 0～40 ℃.Inhale the back seawater and can arrange the sea, can be used as refrigerated sea water, also can be used as the raw material of evaporating brine.
Formerly the potassium ion in the adsorbing seawater saturated after, can feed bittern again and continue absorption, wait to adsorb potassium in the bittern and stop absorption after saturated.Inhale back bittern prepares magnesium salts, bromine as salt chemical engineering raw material.
(2) wash-out
In adsorbing saturated zeolite, feed tap water, the seawater in the zeolite is ejected; In zeolite, feed eluent again, eluent be under the normal temperature preparation contain magnesium chloride and ammonium chloride mixing solutions, eluent contains magnesium chloride 260～300 grams per liters, ammonium chloride 20～50 grams per liters, eluting temperature is at 0～40 ℃.NH in the eluent
4 +With the K on the zeolite
+Wash, obtain rich potassium mother liquor, potassium type zeolite becomes ammonium type zeolite.
Wash-out is inhaled the eluent+KZ → rich potassium mother liquor+NH of saspachite
4Z
K in the rich potassium mother liquor
+Than enrichment in the seawater more than 30 times.Only adsorb in seawater, wash-out makes and contains K
+12.01-13.40 the rich potassium mother liquor of grams per liter; With seawater and sea water bittern absorption, wash-out makes and contains K
+19.50-21.45 the rich potassium mother liquor of grams per liter.
(3) regeneration
With sodium chloride solution ammonium type zeolite is converted into na-pretreated zeolite, and obtains ammonium salt-containing water, the recyclable ammonium of ammonium salt-containing water or as soda factory system alkali raw material.
Sodium salt solution+NH
4Z → ammonium salt-containing water+NaZ
Sodium chloride solution is to utilize Industrial Salt to add the saturated brine that water is made, and saturated brine concentration is NaCl 300～320 grams per liters, and regeneration temperature is an outside temperature, and its temperature range is at 0～40 ℃.
(4) evaporation concentration
The rich potassium mother liquid evaporation that above-mentioned wash-out is made concentrates, and the evaporation final temperature is 126～128 ℃.The vapour phase of evaporation is a water vapour, has solid-phase chlorination sodium to separate out in the evaporative process.Water vapour is the thermal source of next effect in multiple-effect evaporation, being used to of water vapor condensation gained water of condensation salt, and the end is imitated water vapour and is entered mixing condenser and water coolant mixing and discharge.
(5) insulation sedimentation
Above-mentioned complete evaporation of liquid under 100～105 ℃ of conditions, is incubated sedimentation 2 hours.Solid-phase chlorination sodium is deposited in lower floor's salt slurry, and the upper strata is the clear liquor that contains Repone K, magnesium chloride.
(6) crystallisation by cooling
To be incubated settled clear liquor stirring and be cooled to 25～35 ℃, carnallitite (KClMgCl in the process of cooling
26H
2O) separate out with solid phase form.
(7) centrifugation
Above-mentioned refrigerative is finished the liquid sedimentation, and lower floor is the carnallitite slurry, and the upper strata is a magnesium chloride solution.The carnallitite slurry gets carnallitite and magnesium chloride solution through centrifugation; Magnesium chloride solution adds ammonium chloride and makes eluent.
(8) decompose washing
According to carnallitite: the quality ratio is 1: 0.433 a ratio, adds water in carnallitite, solves thick potassium slurry through stirring to divide; The centrifugation of thick potassium slurry gets thick potassium and decomposed solution, and by thick potassium: the quality ratio is that 1: 0.80 ratio adds water in thick potassium, and agitator treating gets smart potassium and starches; Smart potassium slurry gets Repone K and washings through centrifugation.After decomposing the decomposed solution and washings mixing of washing procedure by-product, return the evaporation concentration operation, the rich potassium mother liquor that makes with wash-out carries out evaporation concentration.
The present invention be a kind of be the novel method of raw material production Repone K with seawater and sea water bittern, adopt normal temperature absorption, wash-out and regenerated process of enriching, decomposed solution, washings recycle, and realize utilizing seawater less energy-consumption and low cost to produce Repone K.Self-evaporatint n. is concentrated into and decomposes K in the washing process in this technological cycle test
+The rate of recovery reach 85%, the quality product of Repone K reaches the III class acceptable end product standard of GB 6549-1996 Repone K.
Description of drawings
Fig. 1 produces the schema of Repone K for seawater
Embodiment
Embodiment 1
Get six glass exchange columns (15 * 1410 millimeters of φ), every post filling zeolite 200 grams, about 1150 millimeters of zeolite loading height.Above-mentioned six zeolite column series connection is used, got somewhere, Tianjin seawater, its seawater component is as follows: K
+0.38 grams per liter, Ca
2+0.390 grams per liter, Mg
2+1.220 grams per liter, Cl
-18.360 grams per liter.Above-mentioned seawater is fed the zeolite exchange post, and the flow rate control of seawater in the zeolite exchange post is in 70 ml/min, and feeding the seawater amount is 116 liters, K in the seawater of absorption back
+0.167 grams per liter, this moment, zeolite adsorbed saturated substantially.Finish the absorbing unit operation, the zeolite after absorption is finished becomes the potassium type by the sodium type.
The mixing solutions that preparation contains magnesium chloride and ammonium chloride is an elutriant, and its concentration is: NH
4Cl27.32 grams per liter, MgCl
2280 grams per liters, H
2O 959.40 grams per liters.To carry out wash-out in 1200 milliliters the above-mentioned elutriants feeding zeolite column, the flow rate control of elutriant in zeolite column is in 20 ml/min.Wash-out can get 1200 milliliters of rich potassium mother liquors, and rich potassium mother liquor consists of: KCl 25.6 grams per liters, MgCl
2280 grams per liters, NH
4Cl 8.90 grams per liters, NaCl 20 grams per liters.After wash-out was finished, potassium type zeolite became ammonium type zeolite.
The preparation saturated nacl aqueous solution, sodium chloride concentration is NaCl 320 grams per liters, H
2O 890 grams per liters.To regenerate in the zeolite column behind 3600 milliliters of saturated nacl aqueous solutions feeding wash-outs.The flow rate control of saturated nacl aqueous solution in zeolite column be in 20 ml/min, and regeneration gained solution is referred to as regenerated liquid, regenerated liquid consist of NH
4 +8.65 grams per liter, K
+1.71 grams per liter, Na
+113.75 grams per liter.After regeneration was finished, ammonium type zeolite became na-pretreated zeolite, is used for the absorption process that " absorption-wash-out-regeneration " carried out in next circulation.
With above-mentioned 1200 milliliters (1540 gram) rich potassium mother liquor heating evaporations in vaporizer, stop heating when being evaporated to 126 ℃, vaporize water 570 grams get complete evaporation of liquid 970 grams.
The beaker that fills complete evaporation of liquid is covered completely with watch-glass, put into 100 ℃ of baking oven insulation sedimentations 2 hours.
With settled salt slurry filtered while hot, get solid-phase chlorination sodium 10 grams again.Settled supernatant liquid and filtrated stock are cooled off under stirring condition, when cooling temperature reaches 25 ℃, stop cooling.With the pulp centrifuged separation of above-mentioned cooling, separate to such an extent that solid phase carnallitite 125 restrains, magnesium chloride solution 835 grams (628 milliliters).Carnallitite consists of: MgCl
232.10%, KCl 22%, NH
4Cl 8%, NaCl 5%.Magnesium chloride solution consists of: MgCl
2471.10 grams per liter, KCl 5.13 grams per liters, NH
4Cl 1.08 grams per liters, NaCl 12.3 grams per liters.
Get 120 gram carnallitites and add water 52 grams, stir and decomposed 10 minutes, again its feed liquid centrifugation is got thick potassium 50.1 grams, 100 milliliters of decomposed solution (121.9 gram).Thick potassium consists of: MgCl
213.65%, KCl 49.80%, NH
4Cl 9%, NaCl 10%.Decomposed solution consists of: MgCl
2316.8 grams per liter, KCl 14.50 grams per liters, NH
4Cl 50.90 grams per liters, NaCl24.90 grams per liter.
Get the thick potassium of 50 grams and add water 40 grams, agitator treating 10 minutes gets its feed liquid solid-liquid centrifugation smart potassium 21 grams again, 60 milliliters of washingss (69 gram).Smart potassium consists of: MgCl
21.08%, KCl 91.0%, NH
4Cl 1.0%, NaCl 1.50%.Washings consists of: MgCl
2110 grams per liters, KCl 89 grams per liters, NH
4Cl 71.50 grams per liters, NaCl 78.08 grams per liters.The decomposed solution and the washings of by-product in decomposing washing process evaporate in order to mix with rich potassium mother liquor that next circulation produces.
Embodiment 2
Get six glass exchange columns (15 * 1410 millimeters of φ), every post filling zeolite weight 200 grams, about 1150 millimeters of zeolite loading height.Above-mentioned six zeolite column series connection is used, got somewhere, Tianjin seawater, its seawater component is as follows: K
+0.38 grams per liter, Ca
2+0.390 grams per liter, Mg
2+1.220 grams per liter, Cl
-18.360 grams per liter.Above-mentioned seawater is fed the zeolite exchange post, and the flow rate control of seawater in the zeolite exchange post is in 70 ml/min, and feeding the seawater amount is 110 liters, K in the seawater of absorption back
+0.165 grams per liter, this moment, zeolite adsorbed saturatedly substantially, finished absorbing unit operation, and zeolite became the potassium type by the sodium type after absorption was finished.
The mixing solutions that preparation contains magnesium chloride and ammonium chloride is an elutriant, and its concentration is: NH
4Cl27.32 grams per liter, MgCl
2280 grams per liters, H
2O 959.40 grams per liters.To carry out wash-out in 1200 milliliters the above-mentioned elutriants feeding zeolite column, the flow velocity of control elutriant in zeolite column is 20 ml/min.Wash-out can get 1200 milliliters of rich potassium mother liquors, and rich potassium mother liquor consists of: KCl23.1 grams per liter, MgCl
2280 grams per liters, NH
4Cl 10.74 grams per liters, NaCl 20 grams per liters.After wash-out was finished, potassium type zeolite became ammonium type zeolite.
The preparation saturated nacl aqueous solution, sodium chloride concentration is NaCl 320 grams per liters, H
2O 890 grams per liters.To regenerate in 3600 milliliters of saturated nacl aqueous solutions feeding zeolite column.Flow rate control in the saturated nacl aqueous solution feeding zeolite column is in 20 ml/min, and regeneration gained solution is referred to as regenerated liquid.Regenerated liquid consist of NH
4 +8.65 grams per liter, K
+1.71 grams per liter, Na
+113.75 grams per liter.After regeneration was finished, zeolite became the sodium type by the ammonium type, is used for the absorption process that " absorption-wash-out-regeneration " carried out in next circulation.
Get the rich potassium mother liquor of 1200 milliliters (1540 grams), its composition is KCl 23.1 grams per liters, MgCl
2280 grams per liters, NH
4Cl 10.74 grams per liters, NaCl 20 grams per liters.With rich potassium mother liquor heating evaporation in vaporizer, stop heating when being evaporated to 128 ℃, vaporize water 580 grams get complete evaporation of liquid 960 grams.
The beaker that fills complete evaporation of liquid is covered completely with watch-glass, put into 100 ℃ of baking oven insulation sedimentations 2 hours.
With settled salt slurry filtered while hot, get solid-phase chlorination sodium 10 grams, its clear liquor and filtrated stock are cooled off under stirring condition, when cooling temperature reaches 25 ℃, stop cooling.Gained is cooled off pulp centrifuged separation, separate to such an extent that solid phase carnallitite 130 restrains, magnesium chloride solution 830 grams (625 milliliters).Carnallitite consists of: MgCl
232.50%, KCl 20%, NH
4Cl 8%, NaCl 5%.Magnesium chloride solution consists of: MgCl
2470.00 grams per liter, KCl2.75 grams per liter, NH
4Cl 3.98 grams per liters, NaCl 22.4 grams per liters.
Get 120 gram carnallitites and add water 52 grams, stir and decomposed 10 minutes, its feed liquid centrifugation is got thick potassium 50.1 grams, 100 milliliters of decomposed solution (121.9 gram).Thick potassium consists of: MgCl
214.61%, KCl 41.01%, NH
4Cl 9%, NaCl 7.01%.Decomposed solution consists of: MgCl
2316.8 grams per liter, KCl 34.50 grams per liters, NH
4Cl 50.90 grams per liters, NaCl 24.90 grams per liters.
Get the thick potassium of 50 grams and add water 40 grams, agitator treating 10 minutes gets smart potassium 21 grams with its feed liquid centrifugation, 60 milliliters of washingss (69 gram).Smart potassium consists of: MgCl
21.08%, KCl 91.0%, NH
4Cl 1.0%, NaCl 1.50%.Washings consists of: MgCl
294.63 grams per liter, KCl 45.83 grams per liters, NH
4Cl 57.50 grams per liters, NaCl 42.90 grams per liters.The decomposed solution and the washings of by-product in decomposing washing process evaporate in order to mix with rich potassium mother liquor that next circulation produces.
Embodiment 3
Get six glass exchange columns (15 * 1410 millimeters of φ), every post filling zeolite weight 200 grams, about 1150 millimeters of zeolite loading height.Above-mentioned six zeolite column series connection is used, got somewhere, Tianjin seawater, its seawater component is as follows: K
+0.38 grams per liter, Ca
2+0.390 grams per liter, Mg
2+1.220 grams per liter, Cl
-18.360 grams per liter.Above-mentioned seawater is fed the zeolite exchange post, and the flow rate control of seawater in the zeolite exchange post is in 70 ml/min, and feeding the seawater amount is 120 liters, K in the seawater of absorption back
+0.170 grams per liter, this moment, zeolite adsorbed saturated substantially.Speed with 20 ml/min feeds 2400 milliliters in bittern (bittern) in zeolite column, bittern (bittern) composition is as follows: K
+15.41 grams per liter, Mg
2+52.89 grams per liter, Cl
-170 grams per liters.Finish the absorbing unit operation, after absorption was finished, zeolite became potassium type zeolite by the sodium type.
Preparation contains magnesium chloride and the ammonium chloride mixing solutions is an elutriant, and its concentration is: NH
4Cl 37 grams per liters, MgCl
2270 grams per liters, H
2O 959.40 grams per liters.To carry out wash-out in 1200 milliliters the above-mentioned elutriants feeding zeolite column, the flow rate control of control elutriant in zeolite column is in 20 ml/min, and wash-out can get 1200 milliliters of rich potassium mother liquors, and rich potassium mother liquor consists of: KCl 39.50 grams per liters, MgCl
2270 grams per liters, NH
4Cl 10.6 grams per liters, NaCl 22 grams per liters.After wash-out was finished, zeolite became ammonium type zeolite by potassium type zeolite.
The preparation saturated nacl aqueous solution, sodium chloride concentration is NaCl 320 grams per liters, H
2O 890 grams per liters.To regenerate in 3600 milliliters of saturated nacl aqueous solutions feeding zeolite column.The control flow velocity of saturated nacl aqueous solution in zeolite column regenerated in 20 ml/min, and regeneration gained solution is referred to as regenerated liquid, regenerated liquid consist of NH
4 +8.65 grams per liter, K
+1.71 grams per liter, Na
+113.75 grams per liter.After regeneration was finished, zeolite became na-pretreated zeolite by the ammonium type, was used for the absorption process operation that " absorption-wash-out-regeneration " carried out in next circulation.
Get the rich potassium mother liquor of 1200 milliliters (1540 grams), it consists of: KCl 39.50 grams per liters, MgCl
2270 grams per liters, NH
4Cl 10.6 grams per liters, NaCl 22 grams per liters.With above-mentioned rich potassium mother liquor heating evaporation in vaporizer, stop heating when being evaporated to 128 ℃, vaporize water 590 grams get one section complete evaporation of liquid, 910 grams.
The beaker that fills complete evaporation of liquid is covered completely with watch-glass, put into 100 ℃ of baking oven insulation sedimentations 2 hours.
With settled salt slurry filtered while hot, get solid-phase chlorination sodium 13 grams, supernatant liquid and filtrated stock are cooled off under stirring condition, when cooling temperature reaches 25 ℃, stop cooling.With the pulp centrifuged separation of above-mentioned cooling, get solid phase carnallitite 215 grams, carnallitite consists of: MgCl
232.70%, KCl 21.50%, NH
4Cl 5.6%, NaCl 5.5%; Magnesium chloride solution 682 grams (520 milliliters), magnesium chloride solution consists of: MgCl
2487.90 grams per liter, KCl 2.25 grams per liters, NH
4Cl 1.31 grams per liters, NaCl 3.02 grams per liters.
Get 210 gram carnallitites and add water 91 grams, stir and decomposed 10 minutes, above-mentioned feed liquid centrifugation is got thick potassium 88 grams, thick potassium consists of: MgCl
213.65%, KCl 49.80%, NH
4Cl 9%, NaCl 10%; Get 180 milliliters of decomposed solution (213 gram), decomposed solution consists of: MgCl
2363 grams per liters, KCl 13.72 grams per liters, NH
4Cl 21.44 grams per liters, NaCl15.28 grams per liter.
Get the thick potassium of 80 grams and add water 63 grams, agitator treating 10 minutes gets smart potassium 35 grams with above-mentioned feed liquid centrifugation, and smart potassium consists of: MgCl
21.10%, KCl 91.2%, NH
4Cl1.2%, NaCl 1.30%; Get 98 milliliters of washingss (111 gram), washings consists of: MgCl
2107.5 grams per liter, KCl 80.8 grams per liters, NH
4Cl 69.18 grams per liters, NaCl 77.04 grams per liters.The rich potassium mother liquor that the decomposed solution of by-product and washings and next circulation produce in decomposing washing process mixes the recyclable Repone K wherein of evaporation.
Claims (7)
1. a method of utilizing seawater to produce Repone K is characterized in that: with the potassium in the natural zeolite adsorbing seawater; With the magnesium chloride solution that contains ammonium chloride is that eluent normal temperature wash-out is inhaled saspachite, make the rich potassium mother liquor that contains potassium, magnesium, ammonium, chlorion, eluent contains magnesium chloride 260～300 grams per liters, ammonium chloride 20～50 grams per liters, eluting temperature is 0～40 ℃, will adsorb that seawater ejects in the natural zeolite after saturated before the wash-out earlier with tap water; Rich potassium mother liquid evaporation concentrates, and complete evaporation of liquid cooling, centrifugation get carnallitite and magnesium chloride solution; Carnallitite adds water decomposition and gets Repone K.
2. the method for utilizing seawater to produce Repone K according to claim 1, it is characterized in that: the magnesium chloride solution through containing ammonium chloride carries out the wash-out zeolite of wash-out, feed saturated brine and regenerate, saturated brine concentration is NaCl 300～320 grams per liters, and regeneration temperature is 0～40 ℃; The feeding saturated brine ejects the magnesium chloride solution that contains ammonium chloride in the natural zeolite with tap water earlier before regenerating.
3. the method for utilizing seawater to produce Repone K according to claim 1 is characterized in that, the spissated final temperature of rich potassium mother liquid evaporation is 126～128 ℃.
4. the method for utilizing seawater to produce Repone K according to claim 1 is characterized in that, it is 25～35 ℃ that rich potassium mother liquid evaporation is finished liquid refrigerative final temperature.
5. the method for utilizing seawater to produce Repone K according to claim 1 is characterized in that, cooling is finished liquid and got carnallitite and magnesium chloride solution through sedimentation, centrifuge dewatering.
6. the method for utilizing seawater to produce Repone K according to claim 1 is characterized in that, carnallitite adds the process that water decomposition gets Repone K and is: with carnallitite: the quality ratio is 1: 0.433 ratio adds water in carnallitite, solve thick potassium slurry through stirring to divide; The centrifugation of thick potassium slurry gets thick potassium and decomposed solution, and by thick potassium: the quality ratio is that 1: 0.80 ratio adds water in thick potassium, and agitator treating gets smart potassium and starches; Smart potassium slurry gets solid-phase chlorination potassium and washings through centrifugation; The centrifuge dehydration of solid-phase chlorination potassium gets product Repone K, and decomposed solution is the solution that contains Repone K, magnesium chloride.
7. the method for utilizing seawater to produce Repone K according to claim 7 is characterized in that, carnallitite adds water decomposition and gets decomposed solution in the Repone K process and washings and mix the rich potassium mother liquor that the back makes with aforementioned wash-out and carry out evaporation concentration.
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| CN102145901B (en) * | 2010-02-08 | 2013-01-09 | 中国科学院过程工程研究所 | Method for recovering ammonium chloride by preparing complex salt of magnesium ammonium chloride hexahydrate |
| CN102068958B (en) * | 2010-12-01 | 2012-12-12 | 河北工业大学 | High-efficiency granulous potassium sorbent and preparation method thereof |
| CN107188201B (en) * | 2017-06-09 | 2023-12-12 | 北京金隅琉水环保科技有限公司 | Separation system and sodium salt and potassium salt separation method |
| CN108017071B (en) * | 2017-12-08 | 2019-09-17 | 中国科学院青海盐湖研究所 | A method of recycling potassium from the tail washings of industry containing potassium |
| CN107758696B (en) * | 2017-12-08 | 2019-09-17 | 中国科学院青海盐湖研究所 | A method of potassium chloride is prepared from the solid mineral of the magnesium of ammonium containing potassium |
| CN110240178B (en) * | 2018-03-09 | 2021-04-23 | 中国科学院大连化学物理研究所 | Selective molecular adsorption sieve and preparation method thereof |
| CN109626398A (en) * | 2019-02-13 | 2019-04-16 | 青海盐湖工业股份有限公司 | A kind of method of essence potassium slurry concentration dehalogenation |
| CN113184880A (en) * | 2021-04-21 | 2021-07-30 | 武汉工程大学 | Method for separating ammonium chloride and potassium chloride mixture based on three-stage crystallization |
| CN113135580B (en) * | 2021-06-01 | 2023-03-17 | 吉林海资生物工程技术有限公司 | Process for preparing artificial carnallite and potassium chloride by extracting potassium from corn soaking solution |
| CN113620314B (en) * | 2021-08-05 | 2024-04-26 | 吉林海资生物工程技术有限公司 | Method for preparing potassium chloride by extracting potassium from corn soaking liquid |
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| CN1418816A (en) * | 2002-12-26 | 2003-05-21 | 河北工业大学 | Method for prodn. of potassium nitrate by using sea water and ammonium nitrate as raw materials |
| CN1792797A (en) * | 2005-12-28 | 2006-06-28 | 河北工业大学 | Process for preparing potassium sulfate by sea water |
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